CN103698350B - A kind of X-ray double spectrometer - Google Patents
A kind of X-ray double spectrometer Download PDFInfo
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- CN103698350B CN103698350B CN201310726315.XA CN201310726315A CN103698350B CN 103698350 B CN103698350 B CN 103698350B CN 201310726315 A CN201310726315 A CN 201310726315A CN 103698350 B CN103698350 B CN 103698350B
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Abstract
The present invention relates to a kind of X-ray double spectrometer, described pair of spectrometer comprises: 4 kw of power X-ray tubes, three-dimensional sample transfer table, CCD camera, capillary X-ray semi-permeable mirror, X-ray semiconductor detector and electronic system I, flat crystal, NaI? X-ray detector and electronic system II, collimating slit I and collimating slit II; X-ray energy spectrum and wave spectrum have 4 kilowatts of bulky X ray tubes, before capillary X-ray semi-permeable mirror is fixed on X-ray semiconductor detector and electronic system I, capillary X-ray semi-permeable mirror is positioned at sample oblique upper and the X ray of the elemental characteristic energy becoming the theta alignment sample of 67.5 degree to eject for the microregion element collecting sample, and computer-controlled three-dimensional sample transfer table mobile example does interested microcell in line sweep or Surface scan analysis or sample.
Description
Technical field
The present invention relates to a kind of x-ray fluorescence analysis spectrometer, be specifically related to a kind of X-ray double spectrometer.
Background technology
X-ray fluorescence analysis spectrometer is the important analytical approach of constituent content in the various sample of a kind of nondestructive analysis, its principle is that the X-ray beam emitted from x-ray source (such as X-ray tube etc.) is radiated at sample, room is left after the irradiated excitation of X-rays of atomic nucleus inner electron of element contained in sample, extranulear electron inner layer Vacancy Transition, and send the X ray with characteristic energy, X-ray detector accepts the energy of the characteristic X-ray that element in sample sends, through prime amplifier, after the electronic system such as main amplifier and multichannel analyzer, how many differentiations its element kind and constituent content of the characteristic energy that sends of middle element and peak area per sample.X-ray fluorescence analysis spectrometer is generally divided into energy-dispersive X-ray fluorescence (EDXRF) analyzer (abbreviation X-ray energy spectrum) and Wavelength Dispersive X-Ray Fluorescence Analysis (being called for short X ray wave spectrum).Two kinds of all each features of having oneself by oneself of spectrometer.Wherein energy-dispersive X-ray fluorescence (EDXRF) spectrometer analysis speed is fast, and be easy to realize line sweep and Surface scan analysis, but energy resolution is low, power spectrum background is high, and detection limit is high; And Wavelength Dispersive X-Ray Fluorescence Analysis resolution is high, analyze background low, detection limit is low, but analysis speed is slow, is difficult to realize line sweep and Surface scan analysis.
In order to realize the problem that X-ray energy spectrum and wave spectrum are measured simultaneously, the existing two spectrometers possessing energy spectrometer and spectrometer are only a set of XRF power spectrum and a set of X ray wave spectrum are simply combined, it must possess two X-ray tubes and two X-ray detectors simultaneously, equipment is complicated, overall volume is huge, price is high, and existing pair of spectrometer also cannot to tiny area analysis specific in short grained sample or sample in addition, and accuracy of detection is limited.Although application number is 200810116613.6 and 200920145676.4 all propose the analysis utilizing Polycapillary X-ray lens to achieve sample microcell, but above-mentioned two parts of patents are all utilize kapillary full impregnated mirror that the X-ray beam that less than 50 watts miniwatt X-ray tubes excite is pooled point, the microcell of deexcitation sample, detector detects the elemental signals of whole film micro area, still power spectrum can not be realized and wave spectrum is analyzed simultaneously, even if realize power spectrum and wave spectrum to analyze and also must increase X-ray tube and corresponding detector on above-mentioned two patent bases simultaneously, the inevitable complicacy still needing increase equipment.
Summary of the invention
In order to solve the defect and problem that exist in above-mentioned prior art, the present invention proposes a kind of based on capillary X-ray semi-permeable mirror X-ray double spectrometer, it can carry out high-precision constituent content mensuration, line scanning and Surface scan analysis can be carried out again simultaneously, also can carry out specific tiny area analysis in short grained sample or sample, equipment is simple.
The present invention is achieved by the following technical solutions:
Described X-ray double spectrometer comprises: 4 kw of power X-ray tubes, three-dimensional sample transfer table, CCD camera, capillary X-ray semi-permeable mirror, X-ray semiconductor detector and electronic system I, flat crystal, NaIX ray detector and electronic system II, collimating slit I and collimating slit II;
Described 4 kw of power X-ray tubes are positioned at the oblique upper in the left side of three-dimensional sample transfer table, become miter angle degree with surface level, and X ray to incide on the sample to be detected on described three-dimensional sample transfer table with the angle of 45 degree by described 4 kw of power X-ray tubes;
Described collimating slit I, collimating slit II, flat crystal and NaIX ray detector and electronic system II are positioned at the oblique upper on the right side of three-dimensional sample transfer table; After flat crystal light splitting, NaIX ray detector and electronic system II is entered through after collimating slit I through collimating slit II from sample excitation elemental characteristic X ray out;
Described capillary X-ray semi-permeable mirror is positioned at the front end of X-ray semiconductor detector and electronic system I, before described capillary X-ray semi-permeable mirror is fixed on X-ray semiconductor detector, 67.5 degree of angles are become with the surface level of sample on the right side of sample, the smaller diameter end of described capillary X-ray semi-permeable mirror aims at described sample film micro area to be detected, and larger diameter end aims at X-ray semiconductor detector and electronic system I; Elemental characteristic X ray enters hollow glass tube in the angle of hollow glass inside pipe wall transmitting total reflection from the smaller diameter end of capillary X-ray semi-permeable mirror to meet, and transmits in the mode of total reflection at the smooth inner wall of hollow glass tube in the inside of glass capillary;
CCD camera is positioned at directly over sample, and computing machine controls described three-dimensional sample transfer table and can move to X, Y and Z tri-directions by mobile example, and CCD camera combines so that find tested film micro area fast.
Further, described 4 kw of power X-ray tubes 1, can realize the content of the vestige element measuring more than 10ppm in sample, can measure more than 30 element.
Further, described X-ray semiconductor detector has the resolution of 130 electron-volts; Described NaIX ray detector has the resolution of more than 500 volts, and NaIX ray detector and flat crystal 6 combine, and resolution can arrive 20 electron-volts.
Further, the diameter of described film micro area 9 is 50-200 micron.
Further, described computing machine is also by controlling the software of CCD camera, computer screen can be observed the situation of sample, the centre bit of the software display of CCD camera is equipped with a red cross, by computer software control three-dimensional sample transfer table 2 mobile example, the tiny area that needs are measured is positioned at the point of crossing of cross, simultaneous computer adjusts the distance of capillary X-ray semi-permeable mirror 4 and testing sample by controlling three-dimensional sample transfer table 2, when the micro-raman spectra of the software observing samples of CCD camera reaches utmost sharpness, show that the distance of kapillary semi-permeable mirror and sample is just right.
Further, described sample is soil, rock, metal stainless steel, cement, pottery, circuit board or other solid-state thick target or Atmospheric particulates.
Further, described element is from boron element to uranium element.
Further, described capillary X-ray semi-permeable mirror 4 is at high temperature merged by the hollow glass tube of 100,000-100 ten thousand internal diameters, 3 microns of-15 microns of inner wall smooths and forms, and the internal diameter of kapillary is uneven, and the caliber ratio entering the kapillary of end goes out to hold caliber thin.
The beneficial effect that the invention provides technical scheme is:
Solve while sample realizes Spectrum Analysis, also can carry out line sweep and the Surface scan analysis of microcell; Two spectrometers of dual-purpose two kinds of functions, can measure the mean value of constituent content in sample, also can measure indivedual values of a certain microcell; Improve the analysis speed of sample, also improve the accuracy of analysis result.
Accompanying drawing explanation
Fig. 1 is X-ray double spectrometer platform structure figure
Fig. 2 is capillary X-ray semi-permeable mirror schematic diagram
Main Reference Numerals illustrates:
1-4 kw of power X-ray tube, 2-three-dimensional sample transfer table, 3-CCD camera, 4-capillary X-ray semi-permeable mirror, 5-X-ray semiconductor detector and electronic system I, 6-flat crystal, 7-NaIX ray detector and electronic system II, 8-collimating slit I, the film micro area that 9-kapillary semi-permeable mirror is collected, 10-collimating slit II.
Embodiment
See accompanying drawing 1, the invention provides a kind of X-ray double spectrometer, X-ray energy spectrum and wave spectrum have 4 kilowatts of bulky X ray tubes 1, before capillary X-ray semi-permeable mirror 4 is fixed on X-ray semiconductor detector, capillary X-ray semi-permeable mirror 4 is positioned at the upper right side of sample together with X-ray semiconductor detector, and become 45 degree of places with the surface level of sample, aim at the X ray of the elemental characteristic energy that sample ejects for microcell (diameter is at the 50-200 micron) element collecting sample, computer-controlled three-dimensional sample transfer table mobile example does line sweep or Surface scan analysis, computing machine is also by controlling the software of CCD camera, computer screen can be observed the situation of sample, the centre bit of the software display of CCD camera is equipped with a red cross, by computer software control three-dimensional sample platform mobile example, the tiny area that needs are measured is positioned at the point of crossing of cross, simultaneous computer also controls the distance of three-dimensional sample transfer table adjustment capillary X-ray semi-permeable mirror 4 and testing sample, when the microcell of CCD observing samples reaches utmost sharpness, show that the distance of kapillary semi-permeable mirror and sample is just right.
Described X-ray semiconductor detector has the resolution of 130 electron-volts; Described NaIX ray detector has the resolution of more than 500 volts, and NaIX ray detector and flat crystal 6, collimating slit I8 and collimating slit II10 etc. combine, and its resolution can arrive 20 electron-volts, therefore has high resolution; Bulky X ray tube is 4 kilowatts simultaneously, can measure the content of the vestige element of more than 10ppm in solid sample, can measure more than 30 element.
Described capillary X-ray semi-permeable mirror 4 such as Fig. 2 is at high temperature merged by the hollow glass tube of 100,000-100 ten thousand internal diameters, 3 microns of-15 microns of inner wall smooths, 67.5 degree of angles are become with the surface level of sample on the right side of sample, elemental characteristic X ray enters hollow glass tube in the angle of hollow glass inside pipe wall transmitting total reflection from the smaller diameter end of capillary X-ray semi-permeable mirror to meet, and transmits with the inside of the mode be totally reflected at glass capillary.Its principle as shown in Figure 2, the regional diameter (50-200 micron) collected determined by the manufacturing process of capillary X-ray semi-permeable mirror and the distance between capillary X-ray semi-permeable mirror and sample, in addition X ray semi-permeable mirror has higher transfer efficiency to energy at the X ray of 0-30 kilovolt than full impregnated mirror, simultaneously, semi-permeable mirror is greater than the X ray of 10 kilovolts up to the transfer efficiency of 30% to energy, further increase the detection accuracy of heavy metal element.
Computer-controlled three-dimensional sample mobile platform can move to X, Y and Z tri-directions by mobile example, and CCD camera combines (pixel 2048 × 2048, enlargement factor 20 times) so that find measured point fast.
This spectrometer can analyze the solid sample of arbitrary size, also can analyze the tiny area of solid sample, and the scope of analytical element can from boron element to uranium element.
The above; be only the preferred embodiment of the present invention; but protection scope of the present invention is not limited thereto; those skilled in the art should understand that; when not departing from by the principle of the present invention of claim and its scope of equivalents thereof and spirit; can to modify to these embodiments and perfect, these amendments and improve also should in protection scope of the present invention.
Claims (8)
1. an X-ray double spectrometer, is characterized in that, described pair of spectrometer comprises:
4 kw of power X-ray tubes (1), three-dimensional sample transfer table (2), CCD camera (3), capillary X-ray semi-permeable mirror (4), X-ray semiconductor detector and electronic system I (5), flat crystal (6), NaIX ray detector and electronic system II (7), collimating slit I (8) and collimating slit II (10);
Described 4 kw of power X-ray tubes (1) are positioned at the oblique upper in the left side of three-dimensional sample transfer table (2), become miter angle with surface level, the X ray that described 4 kw of power X-ray tubes (1) send is with on the sample to be detected of the angular illumination of 45 degree on described three-dimensional sample transfer table (2);
Described collimating slit I (8), collimating slit II (10), flat crystal (6) and NaIX ray detector and electronic system II (7) are positioned at the oblique upper on the right side of three-dimensional sample transfer table (2); The elemental characteristic X ray gone out from sample excitation enters NaIX ray detector and electronic system II (7) through after collimating slit I (8) through collimating slit II (10) after flat crystal (6) light splitting;
Described capillary X-ray semi-permeable mirror (4) is positioned at the front end of X-ray semiconductor detector and electronic system I (5), before described capillary X-ray semi-permeable mirror (4) is fixed on X-ray semiconductor detector, 67.5 degree of angles are become with the surface level of sample on the right side of sample, the smaller diameter end of described capillary X-ray semi-permeable mirror (4) aims at described sample film micro area to be detected (9), and larger diameter end aims at X-ray semiconductor detector and electronic system I (5); X ray enters hollow glass tube in the angle of hollow glass inside pipe wall transmitting total reflection from the smaller diameter end of capillary X-ray semi-permeable mirror (4) to meet, and the mode be totally reflected at the smooth inner wall of hollow glass tube is transmitted in the inside of hollow glass tube;
CCD camera (3) is positioned at directly over sample, computing machine controls described three-dimensional sample transfer table (2) and can move to X, Y and Z tri-directions by mobile example, and CCD camera (3) combines so that find tested film micro area (9) fast.
2. a kind of X-ray double spectrometer as claimed in claim 1, is characterized in that, described 4 kw of power X-ray tubes (1), can realize the content of the vestige element measuring more than 10ppm in sample, can measure more than 30 element.
3. a kind of X-ray double spectrometer as claimed in claim 1, is characterized in that, described X-ray semiconductor detector has the resolution of 130 electron-volts; Described NaIX ray detector has the resolution of more than 500 volts, and NaIX ray detector and flat crystal (6) combine, and resolution can arrive 20 electron-volts.
4. a kind of X-ray double spectrometer as claimed in claim 1, is characterized in that, the diameter of described film micro area (9) is 50-200 micron.
5. a kind of X-ray double spectrometer as claimed in claim 1, it is characterized in that, described computing machine is also by controlling the software of CCD camera, computer screen can be observed the situation of sample, the centre bit of the software display of CCD camera is equipped with a red cross, by computer software control three-dimensional sample transfer table (2) mobile example, the tiny area that needs are measured is positioned at the point of crossing of cross, simultaneous computer is by controlling the distance of three-dimensional sample transfer table (2) adjustment capillary X-ray semi-permeable mirror (4) and testing sample, when the micro-raman spectra of the software observing samples of CCD camera reaches utmost sharpness, show that the distance of kapillary semi-permeable mirror and sample is just right.
6. a kind of X-ray double spectrometer as claimed in claim 1, is characterized in that, described sample is soil, rock, metal stainless steel, cement, pottery, circuit board or other solid-state thick target or Atmospheric particulates.
7. a kind of X-ray double spectrometer as claimed in claim 2, is characterized in that, described element is from boron element to uranium element.
8. a kind of X-ray double spectrometer as claimed in claim 1, it is characterized in that, described capillary X-ray semi-permeable mirror (4) is at high temperature merged by the hollow glass tube of 100,000-100 ten thousand internal diameters, 3 microns of-15 microns of inner wall smooths and is formed, the internal diameter of kapillary is uneven, and the caliber ratio entering the kapillary of end goes out to hold caliber thin.
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| CN104833688A (en) * | 2015-04-20 | 2015-08-12 | 绍兴文理学院 | Underwater in-suit X-ray fluorescence spectrum analysis unevenness effect weakening device |
| CN105158285A (en) * | 2015-08-12 | 2015-12-16 | 深圳市西凡谨顿科技有限公司 | XRF (X-ray fluorescence) equipment and automatic sample positioning and multi-point testing method and device thereof |
| DE102016014213A1 (en) * | 2015-12-08 | 2017-07-06 | Shimadzu Corporation | X-RAY SPECTROSCOPIC ANALYSIS DEVICE AND ELEMENTARY ANALYSIS METHOD |
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| CN113791098B (en) * | 2021-11-16 | 2024-03-26 | 四川大学 | Multi-feature surface analysis device |
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